Method of manufacturing textile fibers or artificial silk.



UNITED STATES PATENT OFFICE.

JULIEN VERMEESCH, OF SCHA ERBEEK, BELGIUM. METHOD OF MANUFACTURINGTEXTILE FIBERS 0R ARTIFICIAL SILK.

Specification of Letters Patent.

Patented Nov. 20, 1906.

Application filed April 9, 1906. Serial No. 310,857.

subject of the King of Belgium, residing at Schaerbeek, Belgium, haveinvented a certain new and useful Method of Manufactur ing TextileFibers or Artificial Silk, of which the following is a specification.

This invention relates to an improved method of manufacturing brilliantor glossy textile fibers by means of solution of cellulose incopper-ammonia.

The invention relates to that kind of manufacture of brilliant fibers inwhich the material is discharged through capillary orifices and passesunder pressure into a preci itating-bath, from which it is removed inorder to be wound on spools, &c.

The object of the invention is to obtain specially supple, brilliant orglossy, and very strong filaments. i

It also has for its object to decrease in the. artificial-silk industrythe elements injuriously affectin the health of the workmen and the duraility of the machinery, and finally to allow a great portion of thechemical agents used for the manufacture and precipitation of filamentsto be recovered for reuse.

The invention chiefly consists in introducing jets of solution ofcellulose escaping from capillary orifices into a precipitating-bathconsisting of acidulated or alkalinized glycerin.

Owing to the combined and simultaneous action of the glycerin and of theacid or of the glycerin and of the alkali, an energetic and quickprecipitation is obtained, acting at once on the whole section of thefilament and enabling textile fibers to be obtained which while beingvery strong and water-resistant have an exceedingly brilliant or glossyappearance. The fibers are translucent and exceedingly silky, surpassinganything it has been possible to obtain up to now. On being dischargedfrom the precipitating-bath the threads are introduced into awashing-bath and for that purpose .are wound on glass spools immersed ina solution of glycerin and water, which dissolves the copper. salts anddecolorizes the filaments. A rinsing in clear water, followed by drying,completes the process of manufacture.

In order to obtain a specially energetic and quick action of theprecipitating liquid and at the same time to increase its mercerizingaction, the precipitating agent is preferably prepared in a specialmanner, which will be now described. To two parts of sulfuric acid(density 1.84) is slowly added one part of pure glycerin. It isimportant to make this mixture very slowly, so as to avoid stronggeneration of heat, which would transform the glycerin partly intoa'crolein and produce secondary products disengaging acrid fumes,blackening the liquid, and rendering it unsuitable for use as aprecipitating-bath. The result of this operation 1s the production ofglycerylmonosulfuric acid, C H '(HO),SO,H. (See Wurtz, first part, page1589.) The liquid is cooled by means of any suitable device, and anequalvolume of water is added to it. .Then the cooling is continued andanother quarter part of glycerin is added. The liquid in question istherefore constituted by thirtyseven and one-half per cent. ofglycerylmonocent. of water, and twenty-five per cent. of

in'g-bath, into which is introduced the solu tion of cellulosedischarged under a strong pressure (one and one-half to two atmospheres)in the shape of threads from capillarytubes with an exceedingly smallsection of passage, (the diameter of the dischargeorifice being as lowas 0.15 or even 0.12 of a millimeter.)

The precipitating action of the solution of glycerylmonosulfuric acid onthe solution of cellulose is very energetic and quick, while thepresence of the last addition of glycerin (not combined and simply insolution) is a special and useful feature. It increases, in fact, themercerizing action of the bath, renders the threadmore supple, andprevents the threads from sticking to each other on the winding-spool,and, moreover, its dissolving action on the-non-reduced oxid of copperis obvious. In view of the rapidity of the precipi'tating. action of themixture on the solution of cellulose in very thin threads it isadvisable; in order to obtain all the desirable results, to remove itfrom the thread as quickly as possible. To that end it is necessary,first of all, to reduce to the strict minimum required the duration ofthe contact of the threads with the precipitating liquid. To that effectthe capillary orifices are prefing liquid in such manner that thedischargeorifices are at a small distance below the level of the li uidin a tank of such capacity as it erably arranged relatively to theprecipitat- .glycerin, and this liquid forms the precipitat- IIO willnot ecome saturated too quickly. Ex-

sulfuric acid, thirty-seven and one-half per perience has shown that byarranging the capillary tubes so that they are immersed to the height ofabout two centimeters the duration of the passage of the filamentsthrough the precipitating liquid is regulated in the most advanta eousmanner; but at the same time the spee of winding of the thread must notbe too great. The thread is wound on-a spool arranged outside the bathat a speed of seventy-five to one hundred revolutions per minute.Secondly, it is necessary to stop 1mmediately on leaving the bath theaction of the lycerylmonosulfuric acid carried away by t e thread, whichis effected by treating the thread with a neutralizing li uid Iconsisting, say, of a solution of chlori of sodium in water. Theglycerin carried away by the threads and that released-actuatethe-solution of the non-reduced oXid of copperand chlorid of sodiumcould be used for the same purpose. Such, for instance, are,-generallyspeaking, all soluble salts of organic acids v and minerals in-whichsulfuric acid canbe substituted for the constituent acidformate,acetate, oxalate, alkaline chlorids, chlorids of alkaline earth, &c. Ifon leaving the chlorid of-sodium bath the spool is not completelydecolorized,'it is submitted to washing in a very dilute solution ofbisulfate of soda,

. ing liquid'constituted byasolutionof glycerylmonosulfuric acid inwater mixed -Witl1 glycerin, and subse uently introducing them into aneutralizing ath consisting ofa soluble salt in which sulfuric acid canbe substituted for the constituent-acid,substantially as set forth.

2. A method of manufacturing glossy textile fibers from a solution ofcellulose in copper-ammonia discharged in the shape of fine jets fromcapillary orifices-consisting in cansing the threads to pass through aprecipitating liquid constituted by a solution of glycerylmonosulfuricacid in water mixed with glycerin, and subse uently introducing theminto a neutralizingath consisting of a solution of sodium chlorid inwater, substantially as set forth. I

3. A method of manufacturing glossy textile fibers from a solution ofcellulose in copper-ammoniadischarged in-the shape of fine jets fromcapillary orifices consistingiincausing the threads to pass throughaprecipitating liquid constituted by a-solution of, glycerylmonosulfuricacid in water mixed with glycerin, and subse uentlyiintroducing theminto a neutralizingath consisting of asoluble salt in which-sulfuricacid canbe=substituted for the constituent acid andxwashing the threadsina diluted solutionof bisulfate of-soda, substantially as set fort V 4.Amethod of manufacturing-glossytextile fibers from a solution ofcellulose in copper-ammonia, discharged in the shape of fine jets fromcapillary orifices consistingiin causing the threads to pass throughzaprecipitating liquid constituted by a solutionoflglycerylmonosulfuricacid in water mixedwith glycerin, and subse uentlyaintroducing them intoa neutralizingath consisting ofiasoluble-salt in whichsulfuric acid canbe substituted-for the constituent acid,-dissolvingithe

